Benzylamine → Benzyl[2-(diethylamino)ethyl]amine

HRID 81456

反応式

HRID 81456 の反応式
Cl.[CH2:2]([N:4]([CH2:8][CH3:9])[CH2:5][CH2:6]Cl)[CH3:3].[CH2:10]([NH2:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(N(CC)CC)C>C(O)(C)(C)C>[CH2:10]([NH:17][CH2:6][CH2:5][N:4]([CH2:2][CH3:3])[CH2:8][CH3:9])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 7504BenzylamineHCID 8471TriethylamineHCID 133631-Chloro-2-(diethylamine)ethane hydrochloride

生成物 1

HCID 296044Benzyl[2-(diethylamino)ethyl]amine収率 47%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

2-(diethylamino)-ethyl chloride hydrochloride (1 g, 5.81 mmol) and benzylamine (1.3 ml, 11.62 mmol) were dissolved in t-butanol (40 ml), triethylamine (3.2 ml, 23.24 mmol) was added thereto, and the resulting solution was refluxed for 12 hours. The solution was cooled to room temperature, and distilled under a reduced pressure to remove the solvent. The resulting solid was removed by filtration under a reduced pressure, and the residual solution was extracted with ethylacetate The separated organic layer was washed with saturated sodium bicarbonate aqueous solution, dried over magnesium sulfate, filtered and distilled under a reduced pressure to obtain the title compound 560 mg (yield: 47%).

後処理

  1. temperaturethe resulting solution was refluxed for 12 hours
  2. distillationdistilled under a reduced pressure
  3. customto remove the solvent
  4. customThe resulting solid was removed by filtration under a reduced pressure
  5. extractionthe residual solution was extracted with ethylacetate The separated organic layer
  6. washwas washed with saturated sodium bicarbonate aqueous solution
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. distillationdistilled under a reduced pressure

出典と根拠

ORDレコード
ord-2aa2f080a6e7462a950dda5e0d915cc8
出典データセット
uspto-grants-2014_09
特許番号
US08846699B2

関連ノート

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